油茶皂素大孔树脂纯化工艺优化及LC/TOF-MS分析

食品科学 ›› 2012, Vol. 33 ›› Issue (16): 7-11.

油茶皂素大孔树脂纯化工艺优化及LC/TOF-MS分析

张新富1,2，朱翔3，刘亚军3，夏涛1,*，杜先锋1，高丽萍3，张德龙4

1.安徽农业大学茶叶生物化学与生物技术教育部、农业部重点实验室 2.青岛农业大学园林园艺学院 3.安徽农业大学生命科学学院 4.安徽农业大学微生物防治安徽省重点实验室

收稿日期:2011-06-29 修回日期:2012-07-07 出版日期:2012-08-25 发布日期:2012-09-07
通讯作者: 张新富 E-mail:zxftea@163.com
基金资助:
国家“十一五”科技支撑项目

Purification by Macroporous Adsorption Resin Chromatography and LC/TOF-MS Analysis of Sasanquasaponin

Received:2011-06-29 Revised:2012-07-07 Online:2012-08-25 Published:2012-09-07

摘要/Abstract

摘要： 以市售低纯度茶皂素粗品为原料，采用AB-8大孔树脂进行纯化，得到最佳纯化工艺为30g/L粗皂素溶液上样，30%乙醇洗脱除去多数色素和部分蛋白等杂质，70%乙醇溶液主要洗脱出茶皂素，油茶皂素的得率为55.5%，纯度提高1.86倍。大孔树脂重复利用8次后，吸附和洗脱效果基本不变，放大试验证明其适合工业化生产。LC/TOF-MS分析表明油茶皂素的分子质量主要集中在1170～1304D之间，并确定了一种油茶皂素的分子式为C58H89O26，同时推测了其结构式。

关键词: 茶皂素, 大孔树脂, LC/TOF-MS

Abstract: AB-8 macroporous resin was used to purify commercial crude sasanquasaponin with low purity. The optimal purification process was determined as follows: 30 g/L crude sample solution was loaded followed by washing the resin with 30% ethanol aqueous solution to remove unwanted impurities including most pigments and partial proteins, and the adsorbed sasanquasaponin was finally eluted with 70% ethanol aqueous solution, resulting in a recovery of 55.5% and a purification factor of 1.86. After eighth repeated use, the adsorption and elution capacities of this resin were unchanged basically. Furthermore, the scale-up experiments demonstrated the suitability for industrial production. The LC-TOF-MS analysis indicated that the molecular weight of the purified sasanquasaponin mainly varied between 1170 and 1304 D. In addition, a sasanquasaponin compound with molecular formula C58H89O26 was identified and its structural formula was deduced.

Key words: sasanquasaponin, macroporous resin, LC/TOF-MS

中图分类号:

TS251.52

张新富1,2，朱翔3，刘亚军3，夏涛1,*，杜先锋1，高丽萍3，张德龙4. 油茶皂素大孔树脂纯化工艺优化及LC/TOF-MS分析[J]. 食品科学, 2012, 33(16): 7-11.

参考文献

[1]
[2].宛晓春．茶叶生物化学[M]．北京: 中国农业出版社, 2003:58-6
[3]胡婕伦, 聂少平, 龚毅, 等.响应曲面法优化茶皂素提取工艺的研究[J].食品科学,2009,30(18):106-109
[4]Yoshikawa M, Morikawa T, Li N, et al.Bioactive Saponins and GlycosidesXXIII.1) Triterpene Saponins with Gastroprotective Effect from the Seeds of Camellia sinensis - Theasaponins E3, E4, E5, E6, and E7 –[J].. Chem. Pharm. Bull,2005,53(12):1559-1564
[5]陈力, 邓泽元, 胡蒋宁, 等.高速逆流色谱分离制备茶粕中茶皂素单体[J].食品科学,2010,31(20):127-131
[6]王武, 方红美, 刘京生, 等.茶叶籽饼粕中茶皂素提取工艺研究[J].食品科学,2008,29(9):230-233
[7]KUO PC, Lin TC, Yang CW.Bioactive Saponin from Tea Seed Pomace with Inhibitory Effects against Rhizoctonia solani[J].J. Agric. Food Chem,2010,58:8618-8622
[8]Wan JB, Zhang QW, Ye WC, et al.Quantification and separation of protopanaxatriol and protopanaxadiol type saponins from Panax notoginseng with macroporous resins[J].Separation and Purification Technology,2008,60:198-205
[9]侯如燕, 宛晓春, 黄继轸.油茶皂苷标准品的制备及定量方法的比较[J].食品与发酵工业,2005,31(8):62-65
[10]屈姝存, 唐明远.油茶皂角苷的纯化与含量测定[J].湖南农业大学学报,1999,25(3):257-259
[11] 李建武. 生物化学实验原理和方法[M]. 北京: 北京大学出版社, 2001
[12]Liu J, Luo JG, Sun Y.A Simple Method for the Simultaneous Decoloration and Deproteinization of Crude Levan Extract from Paenibacillus Polymyxa EJS-3 by Macroporous Resin[J].Bioresource Technology,2010,101:6077-6083
[13]涂云飞, 杨秀芳, 孔俊豪.碱性水饱和正丁醇萃取体系联合大孔树脂纯化茶皂素研究[J].茶叶科学,2010,30(增刊1):556-560
[14]Nie w, Luo JG, Wang XB, Wan X, Kong LY.An insight into enrichment and separation of oleanane-type triterpenoid saponins by various chromatographic materials[J].Separation and Purification Technology,2009,65:243-247
[15]侯如燕, 宛晓春, 黄继轸.采用大孔树脂法纯化油茶皂苷的工艺条件[J].食品与发酵工业,2005,31(2):130-132
[16]Wu QB, Wang Y, Guo ML.Triterpenoid Saponins from the Seeds of Celosia argentea and Their Anti-inflammatory and Antitumor Activities[J].Chem. Pharm. Bull,2011,59(5):-
[17]Jian HL, Liao XX, Zhu LW, et al.Synergism and foaming properties in binary mixtures of a biosurfactant derived from Camellia oleifera Abel and synthetic surfactants[J].Journal of Colloid and Interface Science,2011,359:487-492
[18]Matsui Y, Kobayashi K, Masuda H, et al.Quantitative Analysis of Saponins in a Tea-Leaf Extract and Their Antihypercholesterolemic Activity[J].Biosci. Biotechnol. Biochem,2009,73(7):1513-1519
[19]Yoshikawa M, Morikawa T, Nakamura S, et al.Bioactive saponins and glycosidesXXV. Acylated oleanane-type triterpene saponins from the seeds of tea plant (Camellia sinensis)[J].. Chem. Pharm. Bull,2007,55(1):57-63